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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Determination of ribavirin in chicken muscle by quick, easy, cheap, effective, rugged and safe method and liquid chromatography-tandem mass spectrometry
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Determination of ribavirin in chicken muscle by quick, easy, cheap, effective, rugged and safe method and liquid chromatography-tandem mass spectrometry

机译:快速,简便,廉价,有效,坚固,安全的方法和液相色谱-串联质谱法测定鸡肉中的利巴韦林

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摘要

A new analytical method for the determination of ribavirin in chicken muscle using a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and liquid chromatography-tandem mass spectrometry (LC-MS-MS) was developed and validated. Samples were extracted with acidified methanol (methanol:acetic acid, 99:1, v/v). The extract was further purified by QuEChERS method using primary secondary amine (PSA) and C-18. Finally, the extract was dried by nitrogen under 45 degrees C and reconstituted in water. The separation was performed on a Hypercarb analytical column under a gradient elution. The mobile phase was composed of water buffered with ammonium acetate (2.0 mM) and acetonitrile. The proposed method was validated according to the European Commission Decision 2002/657/EC. The values of the decision limit (CC alpha) and the detection capability (CC beta) were 1.1 and 1.5 mu g/kg, respectively. The mean recoveries of ribavirin ranged from 94.2% to 99.2%. The repeatability (expressed as coefficient of variation, CVr) of the method ranged from 4.5% to 4.9% and the reproducibility (CVR) of the method ranged from 4.8% to 5.4%. The method is demonstrated to be suitable for the determination of ribavirin in chicken muscle in conformity with the current EU performance requirements through validation. The total time required for the analysis of one sample, including sample preparation, was about 45 min. (C) 2016 Elsevier B.V. All rights reserved.
机译:开发并验证了一种新的分析方法,该方法使用QuEChERS(快速,简便,廉价,有效,坚固耐用和安全)方法和液相色谱-串联质谱法(LC-MS-MS)测定鸡肉中的利巴韦林。用酸化的甲醇(甲醇:乙酸,99:1,v / v)萃取样品。提取物通过QuEChERS方法使用伯仲胺(PSA)和C-18进一步纯化。最后,将提取物在45摄氏度下用氮气干燥,并在水中重构。分离是在Hypercarb分析柱上进行梯度洗脱的。流动相由醋酸铵(2.0 mM)和乙腈缓冲的水组成。根据欧洲委员会第2002/657 / EC号决定,对提出的方法进行了验证。判定极限(CC alpha)和检测能力(CC beta)的值分别为1.1和1.5μg / kg。利巴韦林的平均回收率在94.2%至99.2%之间。该方法的重复性(表示为变异系数,CVr)范围为4.5%至4.9%,方法的重现性(CVR)范围为4.8%至5.4%。通过验证,证明该方法适用于测定鸡肌肉中的利巴韦林,符合当前的欧盟性能要求。分析一种样品(包括样品制备)所需的总时间约为45分钟。 (C)2016 Elsevier B.V.保留所有权利。

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